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Sommaire du brevet 2798705 

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L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

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  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 2798705
(54) Titre français: DISPOSITIF D'EMULSIFICATION POUR LA PRODUCTION EN CONTINU D'EMULSIONS ET/OU DE DISPERSIONS
(54) Titre anglais: EMULSIFICATION DEVICE FOR CONTINUOUSLY PRODUCING EMULSIONS AND/OR DISPERSIONS
Statut: Périmé et au-delà du délai pour l’annulation
Données bibliographiques
(51) Classification internationale des brevets (CIB):
(72) Inventeurs :
  • DAHMS, GERD (Allemagne)
  • JUNG, ANDREAS (Allemagne)
  • DOERR, HENDRIK (Allemagne)
(73) Titulaires :
  • CLARIANT PRODUKTE (DEUTSCHLAND) GMBH
(71) Demandeurs :
  • CLARIANT PRODUKTE (DEUTSCHLAND) GMBH (Allemagne)
(74) Agent: SMART & BIGGAR LP
(74) Co-agent:
(45) Délivré: 2017-03-14
(86) Date de dépôt PCT: 2011-05-06
(87) Mise à la disponibilité du public: 2011-11-10
Requête d'examen: 2014-05-23
Licence disponible: S.O.
Cédé au domaine public: S.O.
(25) Langue des documents déposés: Anglais

Traité de coopération en matière de brevets (PCT): Oui
(86) Numéro de la demande PCT: PCT/EP2011/057315
(87) Numéro de publication internationale PCT: WO 2011138438
(85) Entrée nationale: 2012-11-06

(30) Données de priorité de la demande:
Numéro de la demande Pays / territoire Date
10 2010 028 774.1 (Allemagne) 2010-05-07

Abrégés

Abrégé français

L'invention concerne un dispositif d'émulsification, pour la production en continu d'émulsions, de nano-émulsions et/ou de dispersions dotées d'une structure à cristaux liquides, comprenant a) au moins un dispositif mélangeur, b) au moins un dispositif d'entraînement pour un organe agitateur, et c) un dispositif de circulation par composant ou par mélange de composant.


Abrégé anglais

The invention relates to an emulsification device for continuously producing emulsions, nano-emulsions and/or dispersions having a liquid crystalline structure, comprising a) at least one mixing system, b) at least one drive for the stirring element, and c) at least one delivery unit for each component or each component mixture.

Revendications

Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.


- 40 -
Claims
1. An emulsifying device for continuous production of
emulsions or dispersions comprising
a) at least one mixing apparatus comprising
- a rotationally symmetric chamber sealed
airtight on all sides,
- at least one inlet line for introduction of
free- flowing components ,
- at least one outlet line for discharge of the
mixed free-flowing components,
- a stirrer unit which ensures laminar flow and
comprises stirrer elements secured on a
stirrer shaft, the axis of rotation of which
runs along the axis of symmetry of the
chamber and the stirrer shaft of which is
guided on at least one side,
wherein the at least one inlet line is arranged
upstream of or below the at least one outlet
line,
wherein the ratio between the distance between
inlet and outlet lines and the diameter of the
chamber is 2:1,
wherein the ratio between the distance between
inlet and outlet lines and the length of the
stirrer arms of the stirrer elements is
3:1-50:1,
and wherein the ratio of the diameter of the
stirrer shaft, based on the internal diameter
of the chamber, is 0.25 to 0.75 times the
internal diameter of the chamber,
such that the components introduced into the
mixing apparatus via the at least one inlet
line are stirred and continuously transported
by means of

- 41 -
a turbulent mixing area on the inlet side, in
which the components are mixed turbulently by
the shear forces exerted by the stirrer unit,
a downstream percolating mixing area in which
the components are mixed further and the
turbulent flow decreases,
a laminar mixing area on the outlet side, in
which a lyotropic, liquid-crystalline phase is
established in the mixture of the components,
in the direction of the outlet line,
b) at least one drive for the stirrer unit and
c) at least one conveying device per component or
per component mixture.
2. The emulsifying device as claimed in claim 1,
characterized in that the chamber has the shape of
a hollow cylinder, of a frustocone, of a funnel,
of a frustodome or of a shape composed of these
geometric shapes, and wherein the diameter of the
chamber remains constant or decreases from the
inlet line to the outlet line and the stirrer unit
being adapted correspondingly to the shape of the
chamber.
3. The emulsifying device as claimed in claim 1,
characterized in that the ratio between the
diameter of the chamber and the distance between
inlet and outlet lines is in the range from 1:50
to 1:2.
4. The emulsifying device as claimed in claim 1,
characterized in that the ratio of the diameter of
the stirrer shaft based on the internal diameter
of the chamber dK is in the range of 0.3 -
0.7*dK.

- 42 -
5. The emulsifying device as claimed in claim 1,
characterized in that at least one constituent of
the stirrer elements is arranged in parallel and
spaced apart from the inner wall of the chamber.
6. The emulsifying device as claimed in claim 1,
characterized in that the stirrer unit is a full-
blade stirrer or part-blade stirrer or a full-
wire stirrer or a part-wire stirrer or a
combination of these stirrers.
7. The emulsifying device as claimed in any one of
claims 1 to 6, characterized in that the chamber
has at least one baffle which promotes a laminar
flow.
8. The emulsifying device as claimed in claim 1,
characterized in that at least one flow sensor is
arranged in at least one of the lines.
9. The emulsifying device as claimed in claim 1,
characterized in that at least one device for
temperature control is coupled to at least one of
the lines, such that the components, component
mixtures, the emulsions or the dispersions are
coolable or heatable.
10. The emulsifying device as claimed in any one of
claims 1 to 9, characterized in that the drive,
the conveying device and the sensor, and the
device for temperature control are connected to a
control device for the monitoring and control of
the mixing apparatuses, the supply and the removal
of the components, component mixtures, or
emulsions or dispersions, the control device
controlling the system such that the viscosity of
the mixture obtained in the first mixing apparatus
is always greater than or equal to the viscosity
in the downstream mixing apparatus(es) and a
laminar flow of the mixed components is ensured.

Description

Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.


CA 02798705 2012-11-06
WO 2011/138438 - 1 - PCT/EP2011/057315
Emulsification device for continuously producing
emulsions and/or dispersions
The present invention relates to an emulsifying device
for continuous production of emulsions and/or
dispersions. The emulsifying device according to the
invention can be employed both for the production of
conventional classical two-phase emulsions, multiphase
emulsions, such as, for example, multiple emulsions and
dispersions as well as of three-phase emulsions (OW),
which in addition to the disperse oil phase also
contain a liquid crystalline gel network phase, but
also for the production of liquid-crystalline
pearlescent agents, liquid-crystalline self-organizing
systems (gel network phases in OW emulsions) such as,
for example, hair conditioning agents, and also skin
and hair cleansing agents such as shampoos, shower
gels, wax and silicone emulsions and perfluoroether
emulsions etc. The emulsifying device according to the
invention can be employed in the polishing and cleaning
agent industry, the cosmetic industry, pharmacy, dye
industry and paint and varnish industry but also in the
food industry.
From the prior art, apparatuses are known for the
production of emulsions and/or dispersions, which are
usually used for carrying out batchwise processes.
WO 2004/082817 Al discloses an apparatus for the
continuous production of emulsions or dispersions with
exclusion of air, which comprises a mixing apparatus
sealed on all sides, which has supply and removal pipes
for the introduction and discharge of fluid substances
or substance mixtures, and also a stirrer unit, which
allows a stirred introduction into the emulsion or
dispersion without production of cavitation forces and
without high-pressure homogenization.

CA 02798705 2012-11-06
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EP 1 964 604 A2 discloses an apparatus and a process
for the continuous production of a mixture of at least
two fluid phases using a mixing vessel sealed on all
sides, and rotationally symmetric around its
longitudinal axis, at least two inlet lines leading
into the mixing vessel for the introduction in each
case of a fluid phase of at least one outlet line
leading from the mixing vessel for the discharging of a
mixture mixed from these phases and a rotatable stirrer
with vanes for stirring the phases, the axis of
rotation of which is in the longitudinal axis of the
mixing vessel. Using the apparatus according to EP 1
964 604 A2, a controlled elongational flow cannot be
produced and measures are not taken for preventing
turbulence and cavitation forces.
It is the object of the present invention, to provide
an emulsifying device, with the aid of which a
continuous production of emulsions, nanoemulsions
and/or dispersions with liquid-crystalline structure is
made possible.
According to the invention, the object is achieved by
an emulsifying device for continuous production of
emulsions and/or dispersions comprising
a) at least one mixing apparatus comprising
- a rotationally symmetric chamber sealed
airtight on all sides,
- at least one inlet line for introduction
of free-flowing components,
- at least one outlet line for discharge of
the mixed free-flowing components,
- a stirrer unit which ensures laminar flow
and comprises stirring elements secured on
a stirrer shaft, the axis of rotation of
which runs along the axis of symmetry of
the chamber and the stirrer shaft of which
is guided on at least one side,

CA 02798705 2012-11-06
WO 2011/138438 - 3 - PCT/EP2011/057315
wherein the at least one inlet line is arranged
upstream of or below the at least one outlet line,
wherein the ratio between the distance between inlet
and outlet lines and the diameter of the chamber is >>
2:1,
wherein the ratio between the distance between inlet
and outlet lines and the length of a stirrer arm of the
stirrer elements is 3:1 to 50:1,
and wherein the ratio of the diameter of the stirrer
shaft, based on the internal diameter of the chamber,
is 0.25 to 0.75 times the diameter of the chamber,
such that the components introduced into the mixing
apparatus via the at least one inlet line are stirred
and continuously transported by means of
a turbulent mixing area on the inlet side, in
which the components are mixed turbulently by
the shear forces exerted by the stirrer
units,
a downstream percolating mixing area in which
the components are mixed further and the
turbulent flow decreases,
a laminar mixing area on the outlet side, in
which a lyotropic, liquid-crystalline phase
is established in the mixture of the
components,
in the direction of the outlet line,
b) at least one drive for the stirrer unit and
c) at least one conveying device per component or per
component mixture.
The percolating mixing area is the transition area of
the mixture, in which this changes from turbulent flow
to laminar flow. In the percolating area following the
turbulent mixing the viscosity increases, caused either
by constant comminution of the droplets or by formation
of liquid-crystalline phases, and the turbulent flow

CA 02798705 2012-11-06
WO 2011/138438 - 4 - PCT/EP2011/057315
decreases. After reaching the critical Reynolds number,
the mixture passes into a laminar mixing area.
Controlled and energy-efficient severing of the drops
during the mixing process or the formation of liquid-
crystalline phases then occurs in the laminar mixing
area under conditions of elongational flow.
The chamber of the at least one mixing apparatus is
rotationally symmetric and preferably has the shape of
a hollow cylinder. The chamber, however, can also have
the shape of a frustocone, of a funnel, of a
frustodome, or a shape composed of these geometric
shapes, wherein the diameter of the chamber from the
inlet line to the outlet line remains constant or
decreases. The stirrer unit is adapted according to the
shape of the rotationally symmetric chamber.
The diameter of the stirrer shaft dss relative to the
internal diameter of the chamber dk is preferably in the
range 0.25-0.75 x dk and the ratio between the distance
between inlet and outlet lines and the length of the
arms of the stirrer elements is preferably in the range
3:1-50:1, particularly preferably in the range 5:1-
10:1, in particular in the range 6:1-8:1. The unusually
large diameter of the stirrer shaft in relation to the
chamber diameter furthermore has the result that the
distance between stirrer shaft and chamber wall -
designated by the person skilled in the art as the
"flow diameter" - is always so small that no thrombi-
like flow can develop and a laminar flow is ensured.
The ratio of the distance between inlet and outlet line
to the diameter of the chamber at the bottom of the at
least one mixing apparatus is ? 2:1. In one form of the
rotationally symmetric chamber deviating from a hollow
cylinder, the ratio of distance between inlet and
outlet lines to the diameter of the chamber is likewise

CA 02798705 2012-11-06
WO 2011/138438 - 5 - PCT/EP2011/057315
2:1 in the area of the inlet line of the at least one
mixing apparatus.
The mixing apparatus is sealed on all sides and is
operated with exclusion of air. The components to be
mixed are introduced into the chamber of the mixing
apparatus as fluid streams, mixed by means of the
stirrer unit until the mixed components reach the
outlet line and are removed such that no air penetrates
into the chamber of the mixing apparatus. The mixing
apparatus is designed here such that as little dead
space as possible is present. In the putting into
operation of the mixing apparatus, the air contained
therein is displaced completely by the entering
components within a short time, whereby the application
of a vacuum is advantageously uneccessary.
Since the system operates with exclusion of air and the
components to be emulsified are introduced into the
mixing apparatus continuously, the components situated
in the mixing apparatus are continuously transported
away in the direction of the outlet line. The mixed
components flow through the mixing apparatus gradually
starting from the inlet to the outlet.
In the mixing apparatus according to the invention, the
components supplied via the inlet lines firstly migrate
after entry into the chamber through a turbulent mixing
area, in which they are first mixed turbulently by the
shear forces exerted by the stirrer units. In this
connection, the viscosity of the mixed product already
noticeably increases. Further in the direction of the
outlet line, the mixture then migrates through a
"percolating area", in which the viscosity of the
mixture further increases due to further intensive
mixing and the system gradually converts into a self-
organizing system. The turbulences in the flow
prevailing in the mixture gradually decrease with

CA 02798705 2012-11-06
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reaching of the percolating area, and the flow ratios
become increasingly laminar in the direction of the
outlet lines. A lyotropic, liquid-crystalline phase
thereby results in the mixture to the outlet line.
Advantageously, the total energy consumption of the
emulsifying device according to the invention is
extremely low. This low total energy consumption
results from always only small volumes having to be
mixed and temperature-controlled in the mixing
apparatuses in comparison to conventional mixing
processes. In particular, cost-intensive and very
energy-consuming heating and cooling processes are thus
minimized and contribute decisively to the low total
energy consumption. The residence times of the mixture
in the mixing chamber are also very short. With a
production capacity of 1000 kg/h, the residence time is
on average between 0.5 and 10 seconds. It results from
this that the inlet lines and pumps are also of
significantly smaller dimensions and thus also the
drives of the pumps take up significantly less energy.
Advantageously, the favorable ratio between the
distance between inlet and outlet lines and the length
of the arms of the stirrer elements, which is
preferably in the range 3:1-50:1, particularly
preferably in the range 5:1-10:1, in particular in the
range 6:1-8:1, contributes, in connection with the
special wire pipes, to the fact that a particularly
effective torque moment utilization is guaranteed and
thus thorough mixing with minimized energy consumption
of the motor at the same time is achieved.
Furthermore, the unusually large shaft diameter in
relation to the chamber diameter makes it possible that
the stirrer shaft itself can be utilized for product
temperature control, which for its part contributes to

CA 02798705 2012-11-06
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the low total energy consumption of the emulsifying
device according to the invention.
As a result of the favorable ratio of diameter of the
chamber to its height and the stirrer unit optimized
for the maintenance of laminar flow, the power uptake
of the stirrer motor is significantly lower and
contributes decisively to the low total energy
consumption of the apparatus according to the
invention. As a result of the thus, overall, smaller
dimensionable components, a very compact and space-
saving construction is characteristic of the mixing
apparatus according to the invention.
The use of magnetic couplings likewise contributes to
the lowering of the overall energy consumption. Since
the transfer of force here from the motor to the motor
shaft takes place by means of permanent magnets, the
motor only has to apply the energy which is needed for
rotation of the external rotor. The internal rotor with
a fixed stirrer shaft is moved by means of the magnetic
force. A further advantage in connection with a plain
bearing is that a hermetically sealed mixing chamber
can be constructed.
For an optimal emulsifying result and for the avoidance
of dead spaces, chambers that have a rotationally
symmetric shape are employed in the mixing apparatuses
according to the invention. Such rotationally symmetric
shapes are preferably hollow cylinders (Fig. 2 A), but
also a frustocone (Fig. 2 B), funnel (Fig. 2 D),
frustodome (Fig. 2 F), or shapes composed of these
(Fig. 2 C, E), in which, for example, a frustocone-like
area connects to a hollow cylindrical area. The
diameter of the mixing apparatus in this connection
either remains constant from the inlet-side end to the
outlet-side end (Fig. 2 A) or it decreases (Fig. 2 B -
F).

CA 02798705 2012-11-06
WO 2011/138438 - 8 - PCT/EP2011/057315
Particularly preferably, a chamber with the shape of a
hollow cylinder or of a frustocone or with a combined
shape of a hollow cylindrical area and a frustocone-
like area is employed in the mixing apparatus according
to the invention. The frustocone is advantageously
distinguished in that the diameter of the inlet-side
end to the diameter on the outlet-side end continually
decreases, while the diameter of the hollow cylinder
with respect to the axis of rotation is constant.
Advantageously, the chambers of the mixing apparatus
and/or the inlet and outlet lines can be temperature-
controlled together or individually.
The supply of components to the mixing apparatus takes
place by means of at least one inlet line, which is
adapted in diameter to the respective component and its
viscosity and guarantees complete filling with the
respective phase. Preferably, the mixing apparatus
according to the invention has at least two inlet
lines. In the case where pre-mixing is to be carried
out in the mixing apparatus, the mixing apparatus,
however, can also have only one inlet line. The
components to be emulsified or to be dispersed can also
be introduced into a common inlet line, for example, by
means of a Y-shaped connection before they reach the
mixing apparatus. Static pre-mixers or passive mixing
apparatuses known to the person skilled in the art can
optionally be situated in this common inlet line.
Component within the meaning of the invention can be a
pure substance, but also a mixture of various
substances.
The angle of entry of the inlet lines into the mixing
apparatus can in this connection be in the range from
00 to 180 , based on the axis of rotation of the mixing
apparatus. The inlet lines can extend into the chamber

CA 02798705 2012-11-06
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laterally through the jacket surface or from below
through the bottom surface.
The inlet and outlet lines can be connected to the
chamber at any desired height and on any desired
circumference of the jacket surface. To guarantee
optimal mixing with, at the same time, maximum
residence time of the components supplied, and to avoid
dead spaces, the entry height of the inlet line(s) is
preferably situated in the lower third, preferably in
the lower quarter, of the chamber, based on the height
of the chamber. The exit height of the outlet line is
preferably situated in the upper third, preferably in
the upper quarter, of the chamber, based on the height
of the chamber.
The diameter of the outlet line is dimensioned such
that the pressure buildup based on the high viscosity
in the at least one or first mixing apparatus is
minimized, but at the same time it is ensured that the
outlet lines are in each case completely filled with
the mixture.
Some products, such as, for example, three-phase OW
emulsions, liquid-crystalline pearlescent agents, and
lyotropic liquid-crystalline phases of self-organizing
systems, can require the additional delayed addition of
components to the percolating area of the first mixing
apparatus, which is situated above the entry height of
the inlet lines and below the height of the outlet
lines. Therefore additional entry lines can be situated
in this area.
The mixing apparatus can be oriented as desired, such
that the axis of rotation of the stirrer unit can
assume any desired position from horizontal to
vertical. Preferably, however, the mixing apparatus is
not arranged such that the axis of symmetry of the

CA 02798705 2012-11-06
WO 2011/138438 - 10 - PCT/EP2011/057315
chamber is arranged vertically and the inlet lines are
attached here above the outlet lines. Very particularly
preferably, the mixing apparatus is arranged such that
the axis of symmetry of the chamber is arranged
vertically and the inlet lines are attached here below
the outlet lines. The drive motor in this connection
drives the stirrer unit preferably from above, likewise
a drive from below, however, is possible.
Surprisingly, it has turned out that with the geometry
of the mixing apparatus, the diameter of the stirrer
shaft dss relative to the internal diameter of the
chamber dk and the ratio between the distance between
inlet and outlet line and the length of the arms of the
stirrer elements is decisive to ensure an optimal
mixing of the supplied phases. In this connection, it
has turned out that the ratio of the diameter of the
stirrer shaft dss based on the internal diameter of the
chamber dk is preferably in the range 0.25-0.75 x dk,
particularly preferably in the range from 0.3-0.7 x dk,
in particular in the range from 0.4-0.6 x dk, and the
ratio between the distance between the inlet and outlet
line and length of the arms of the stirrer elements is
preferably in the range 3:1-50:1, particularly
preferably in the range 5:1-10:1, in particular in the
range 6:1-8:1.
This unusually large diameter of the stirrer shaft with
respect to the chamber diameter furthermore results in
the distance between stirrer shaft and chamber wall -
also designated by the person skilled in the art as the
"flow diameter" - always being so small that no
thrombi-like flow can develop and a laminar flow is
guaranteed.
It has furthermore turned out that with the geometry of
the mixing apparatus, the ratio between the diameter of
the chamber of the mixing apparatus and the distance

CA 02798705 2012-11-06
WO 2011/138438 - 11 - PCT/EP2011/057315
which the components to be mixed must migrate through
from the inlet to the outlet is crucial to guarantee an
optimal mixing of the phases supplied. It has turned
out in this connection that the ratio of diameter to
the distance between inlet and outlet is preferably in
the range 1:50 to 1:2, preferably from 1:30 to 1:3, in
particular in the range from 1:15 to 1:5. Diameter of
the chamber within the meaning of the invention is the
diameter at the bottom of the chamber.
The ratio of diameter to the distance from inlet and
outlet plays a crucial role for the control of the flow
within the mixing apparatus. The success of
emulsification is guaranteed only if the mixture comes
into the laminar area from the initially turbulent flow
which is present in the lower area of the mixing
apparatus, that is in the area of component supply, via
the "percolating area". An exact delimitation of the
individual areas is not possible here, since the
transition between the respective areas is fluid.
Since different amounts of time are needed for the
formation of the lyotropic liquid-crystalline phase,
depending on the components, the mixing apparatus
length can be adapted depending on the product. The
formation of self-organizing systems is influenced by
the following factors: temperature within the system,
water content, composition of the mixture, flow
profile, shear rate and residence time.
The mixing apparatuses used in the emulsifying device
system and according to the invention are equipped with
stirrer units that guarantee a lamellar flow that
guarantees droplet breakup under laminar elongation
conditions. According to an advantageous embodiment of
the invention, at least one constituent of the stirrer
element is arranged spaced apart and parallel to the
inner wall of the chamber.

CA 02798705 2012-11-06
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Preferred stirrer units are full-blade or part-blade
stirrers or full-wire or part-wire stirrers or a
combination of these.
The droplet breakup under laminar elongation conditions
advantageously leads to an extremely small particle
size distribution around a mean droplet diameter in the
emulsion produced. Very often, the graph of the
particle size distribution has a shape very similar to
a Gaussian curve. The particle sizes that are
achievable using the apparatus according to the
invention are, depending on composition of the emulsion
and/or dispersion, in the range from 50 to 20 000 nm.
The diameter of the stirrer unit ds based on the
internal diameter of the chamber dk is preferably in the
range from 0.99 to 0.6 x dk. The stirrer unit, however,
is at least 0.5 mm removed from the chamber wall.
Preferably, the diameter of the stirrer unit is from
0.6 to 0.7 x dk, particularly preferably from 0.99 to
0.8 x dk.
The diameter of the stirrer shaft dss based on the
internal diameter of the chamber dk is preferably in the
range 0.25-0.75 x dk, particularly preferably in the
range from 0.3-0.7 x dk, in particular in the range from
0.4-0.6 x dk.
This unusually large diameter of the stirrer shaft with
respect to the chamber diameter furthermore results in
the distance between stirrer shaft and chamber wall -
also designated by the person skilled in the art as the
"flow diameter" - always being so small that no
thrombi-like flow can form and a laminar flow is
guaranteed.

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The wire stirrers that can be employed in the apparatus
according to the invention are distinguished in that
wires are attached to the stirrer shaft. It has
surprisingly turned out that with these very good
mixing results and a minimized energy consumption are
achieved if these are bent in the manner of a horseshoe
or of a rectangle with rounded corners and are
connected to the stirrer shaft by their ends.
The arrangement on the shaft can also be different,
depending on the product to be mixed. One or more
horseshoe-shaped or rectangularly bent wires can be
arranged on the stirrer shaft. Either a full-wire
stirrer or a part-wire stirrer can be employed here.
The full-wire stirrer (Fig. 3 C) is characterized in
that it consists of at least two wires that are
horseshoe-shaped or bent into the shape of a rounded
rectangle, which relative to the shaft are attached
opposite one another to the shaft and are connected to
the shaft in the upper and lower area of the shaft. The
wires here are preferably tilted and/or rotated
perpendicular to the middle axis and/or are at an angle
of 00 to 90 , preferably from 0 to 45 , particularly
preferably from 0 to 25 , to the left or right, based
on the axis of rotation. The upper and lower lengths of
the wires can have identical or different lengths. As
many wires as desired can be arranged on the
circumference of the shaft. Further wires or any
desired geometric shapes can be situated in the
resulting hollow space between shaft and wire.
A wire diameter is preferred which maximally lies in
the range of the shaft diameter and minimally does not
fall below 0.2 mm, a wire diameter of at most 150 of
the shaft diameter and minimally 0.5 mm is particularly
preferred, in particular the range from 100 of the
shaft diameter and minimally 1% of the shaft diameter.

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The part-wire stirrer (Fig. 3 D) is characterized in
that it consists of at least two U- or horseshoe-shaped
bent wires, the ends of which are connected to the
shaft at any desired height. The wires here are
preferably perpendicular to the middle axis and/or are
tilted and/or rotated at an angle of 00 to 90 ,
preferably from 00 to 45 , particularly preferably of
0 to 25 , to the left or right based on the axis of
rotation. The upper and lower lengths of the wires
extending radially from the stirrer shaft can have
identical or different lengths. As many wires as
desired can be arranged on the circumference of the
shaft. Further wires or any desired geometric shapes
can be situated in the resulting hollow space between
shaft and wire.
A wire diameter is preferred that maximally is in the
range of the shaft diameter and minimally does not fall
below 0.2 mm, a wire diameter of maximally 15% of the
shaft diameter and minimally 0.5 mm is particularly
preferred, in particular the range from 10% of the
shaft diameter and at least 1% of the shaft diameter.
As a result of the favorable ratio of the diameter of
the chamber to the diameter of the stirrer shaft in
combination with the advantageous wire stirrers, a
particularly effective torque utilization is
guaranteed, that minimizes the force which the stirrer
unit exerts on the components to be mixed, such that
good mixing is achieved with, at the same time,
minimized energy consumption of the motor.
Furthermore, the unusually large shaft diameter with
respect to the chamber diameter makes it possible that
the stirrer shaft itself can be utilized for product
temperature control.

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In addition, full-blade stirrers and part-blade
stirrers have turned out to be particularly suitable.
The full-blade stirrer (Fig. 3 A) is characterized in
that it consists of at least two square, rectangular,
horseshoe-shaped or trapezoidal metal sheets, wherein
the corners of the metal sheets are rounded off to
prevent the production of turbulent flows, wherein one
side is connected to the shaft, and the metal sheets
reach uninterruptedly from the upper area of the shaft
to the lower area of the shaft. The metal sheets in
this connection are preferably perpendicular to the
middle axis and/or are inclined and/or rotated at an
angle of 00 to 900, preferably from 00 to 450,
particularly preferably from 00 to 25 , to the left or
right of the middle axis. The upper and lower edges of
the metal sheets can have identical or different
lengths. As many metal sheets as desired can be
arranged on the circumference of the shaft. The
individual blades can be provided with further
geometric passages, such as bores or die-cuts.
The part-blade stirrer (Fig. 3 B) is characterized in
that it consists of at least two square, rectangular,
horseshoe-shaped or trapezoidal metal sheets, wherein
one side is connected to the shaft at any desired
height. The metal sheets in this connection are
preferably perpendicular to the middle axis and/or are
tilted and/or rotated at an angle of 0 to 90 ,
preferably of 0 to 45 , particularly preferably of 0
to 25 , to the left or right of the middle axis. The
upper and lower edges of the metal sheets can have
identical or different lengths. As many metal sheets as
desired can be arranged on the circumference of the
shaft. The individual metal sheets can be provided with
further geometric passages.

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Further stirrer units known to the person skilled in
the art and their special designs can be installed for
the mixing of the product in the mixing apparatus, such
as, for example, the designs anchor stirrer, dissolver
disk, inter-MIG, etc. Likewise, it is possible to
combine various stirrer designs with one another on one
stirrer shaft.
The stirrer units used in the mixing apparatus
according to the invention are furthermore
distinguished in that each stirrer shaft is guided in a
rotationally stable manner, to this end preferably in
the upper and lower area of the mixing apparatus.
Imbalances in the stirrer unit at high speeds are thus
intended to be ruled out or avoided to the greatest
possible extent, so that turbulence which affects or
even prevents the buildup of the necessary laminar flow
cannot be generated. Ball bearings, linear ball
bearings, plain bearings, linear plain bearings or the
like, for example, can be used for guiding the shaft.
The shaft is advantageously balanced for further
rotational stability.
The materials from which both the mixing apparatus
itself and the above-mentioned stirrer designs, in
particular the above-mentioned full-blade stirrers,
part-blade stirrers, full-wire stirrers and part-wire
stirrers are manufactured are suited to the chemical
properties of the components to be emulsified and the
resulting emulsions. Preferably, the stirrer units in
the mixing apparatus according to the invention
comprise steels, such as, for example, stainless
steels, but also construction steels, plastics, such
as, for example, PEEK, PTFE, PVC or plexiglass or
compound materials or combinations of steel and
plastic.

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The mixing apparatuses are conceived such that they
spontaneously oppose only a small counter pressure from
the components to be emulsified. It is achieved by
means of the specially bent wire stirrers that even
during the mixing process only a minimal pressure
buildup results. For this reason, the mixing apparatus
can essentially be designated a pressureless/low-
pressure system.
To achieve this, the cross-section of the outlet line
must be chosen such that the total amount of product of
the mixed components can flow off unhindered. In this
connection, especially in the mixing apparatus 1, the
extreme viscosity increase is to be observed, which
results in the buildup of the highly viscous lyotropic
liquid-crystalline gel phase. In the dimensioning of
further process technology components, such as, for
example, pipelines, heat exchangers etc., care is to be
taken that these are only oppose minimal pressure
decreases to the entire system in order to guarantee a
continuous low-pressure system. Depending on product
and apparatus configuration, pressure decreases of
below 0.5 bar can be realized in the entire system.
In the emulsifying device according to the invention,
temperature control of the mixing apparatus and the
inlet and outlet lines is advantageously particularly
simply and effectively realizable. On account of the
small volumes and the large ratio of surface to volume
of the chamber in the mixing apparatus caused by the
shape of the chamber, a better controlled temperature
management of the product can be guaranteed in the
apparatus according to the invention in comparison to
conventional emulsifying devices.
For heating the mixing apparatuses, a double jacket is
particularly suitable. This can be heated with gases,
such as, for example, steam, or with liquids, such as,

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for example, water or thermal oil. Further
possibilities are, for example, electrical heating such
as heating wires, heating cables or heating cartridges.
For the temperature control of the components to be
emulsified in the chamber and in the inlet and outlet
lines, both passive heat exchange processes, such as,
for example, cooling ribs, active processes, such as,
for example, tube bundle heat exchangers, and also
combinations of both methods can be employed to
guarantee temperature control as uniform and rapid as
possible.
For the temperature control of the components to be
emulsified from outside to inside, the mixing apparatus
is preferably equipped with a double jacket, full- or
half-tube cooling coils, which are attached outside
and/or inside the mixing apparatus and are fed with a
cooling/heating medium, e.g. by means of a thermostat.
Preferably, the temperature control is improved by
additional baffles in the interior of the double
jacket. By means of the optimization of the ratio of
diameter to the distance between inlet and outlet line,
it is additionally possible to adjust the flow rate of
the mixed material such that an optimal temperature
exchange is afforded.
The device according to the invention is distinguished
in contrast to conventional batch processes in that
basically not all components of the recipe have to be
heated, but that only those components that are not
sufficiently fluid at room temperature are heated until
they are fluid. The embodiment of the mixing
apparatuses according to the invention, in particular
the length/diameter ratio, is advantageous for the heat
control, such that the energy dissipated by stirring
can be utilized in controlled heat supply.

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In a further embodiment, the mixing apparatus according
to the invention is equipped with baffles, which
promote a lamellar flow of the components.
According to an advantageous embodiment, the baffles
and/or the stirrer unit can be temperature controlled
and thus make possible temperature control of the
mixture.
Preferably, the at least one mixing apparatus comprises
a rotationally symmetric chamber, in which the
components to be emulsified are converted to a
lyotropic liquid-crystalline phase by passing through a
turbulent and a percolating area.
In a further embodiment of the invention, the at least
one mixing apparatus comprises a plurality of
rotationally symmetric chambers connected in series. It
is thus made possible that, if for construction reasons
the height of the at least one mixing apparatus is
restricted, the mixing process can be divided in a
number of successive chambers. The components here do
not pass through the three different areas, turbulence
area, percolating area and laminar area within a single
chamber, but within a number of chambers.
The emulsifying device according to the invention in
the simplest case comprises the at least one mixing
apparatus corresponding to the aforementioned
description.
Customarily, an emulsifying device according to the
invention, however, comprises at least two mixing
apparatuses, which are connected in series one behind
the other and into which various components are fed and
mixed with one another in succession or simultaneously.
Here, the viscosity of the mixture produced in the

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first mixing apparatus is always greater than or equal
to the viscosity in the following mixing apparatus(es).
At least the first mixing apparatus must here
correspond in construction and function to the at least
one mixing apparatus, i.e. in the first mixing
apparatus the particular flow control must be
guaranteed, in which the components are first mixed
turbulently and then achieve a lyotropic liquid-
crystalline state by means of passing through a
percolating area.
In the production of conventional two-phase systems
such as WO emulsions, but also OW emulsions without a
gel network phase, in the emulsifying device according
to the invention the ratio of internal (disperse) phase
and external (continuous) phase in the first mixing
apparatus is always greater than in the following
mixing apparatus(es).
In the emulsifying device according to the invention,
it is further possible that a number of mixing
apparatuses can be connected not only in series one
behind the other, but also serially above or under one
another. Here, the individual mixing apparatuses can
also be accommodated together in a housing, such that
the separation of the mixing apparatuses is not visible
from outside.
In the further course of the production of the said
products in. the emulsifying device according to the
invention, the highly viscous content of the first
mixing apparatus is led into the following mixing
apparatus(es). Here, the supply in the following mixing
apparatuses is arranged such that the height of the
entry lines preferably takes place in the lower third,
preferably in the lower quarter, based on the height of
the mixing apparatus.

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In the mixing apparatuses connected downstream of the
first mixing apparatus, it is no longer necessary that
the internal phase predominates in proportion to the
continuous phase. In one embodiment of the emulsifying
device according to the invention, in a first mixing
apparatus the components to be emulsified are converted
to a laminar liquid-crystalline phase and in a second
mixing apparatus diluted to the desired concentration
by the addition of external phase.
The emulsifying device according to the invention also
comprises appropriate peripherals, such as
storage containers for at least 2 components
connecting lines for the supply of the components to
the at least one mixing apparatus, associated pumps and
valves,
connecting lines for the removal of components,
control device for monitoring and regulation of the
process stages,
a display device with an operating part for the
visualization and input of process variables.
Mixing apparatuses and connecting lines are
temperature-controllable.
Mixing apparatus and connecting lines can have sensors
for product and process control.
Furthermore, the outlet lines of the individual mixing
apparatuses can have further sensors, that make
possible, for example, a continuous particle size
measurement, directly or in a bypass, a temperature
measurement, a pressure measurement, a conductivity
measurement, a viscosity measurement, or the like.

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The product quality of the final product is
preferentially determined in the device according to
the invention in the first stirring stage.
Furthermore, in the inlet and outlet line of the mixing
apparatuses according to the invention or in a number
of mixing apparatuses, a heat exchanger can be attached
between the mixing apparatuses of a system according to
the invention. It has been shown that here the
introduction of tube bundle heat exchangers in
combination with perforated baffles in the product
stream and baffles in the heating and cooling circuit
is very effective. As a result of the comparatively
small product amounts, advantageously a very compact
and efficient construction of the heat exchangers is
possible. These heat exchangers can be employed both in
the serial method of construction and in the method of
construction connected in series. The introduction of
other heat exchanger construction forms, such as, for
example, cooling coils, tube bundle heat exchangers,
double tube heat exchangers, ribbed tube heat
exchangers, spiral belt heat exchangers, plate heat
exchangers, store heat exchangers and other special
designs, is likewise possible.
As a cooling medium, both gases, such as, for example,
nitrogen, and also liquids, such as, for example, water
or thermal oil, can be employed.
Using the above-mentioned heat exchangers, it is
likewise possible to cool and also to heat. Here too, a
suitable heating/cooling for the desired product can be
chosen by the person skilled in the art.
Depending on the use of the emulsifying device, a
combination of heating and cooling units is optionally
also possible. This can also be simply and efficiently

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solved as described above by use of a double jacket, a
heating/cooling coil or an appropriate heat exchanger.
In smaller emulsifying devices, particularly suitable
for this are heating/cooling baths (thermostats), which
preferably are monitored and operated by an overriding
control. Additionally, a stand-alone operation can also
be made possible using these thermostats. Since the
thermostats as a rule also have the possibility of
attaching an external temperature sensor, this can be
introduced into the product flow. The thermostat then
independently controls the heating or cooling capacity
needed and thus provides for an optimum product
temperature. A further advantage of this method is a
release of the control, since this can leave the
regulation of the temperature of the mixing apparatuses
to the thermostat.
By means of optimization of the temperature of the
component supply in the mixing apparatuses,
optimization of the product temperature can likewise be
achieved. In this connection, the inlet path of the
components from the storage container to the entry into
the mixing apparatus can also be optimized and utilized
to the extent that component streams arrive in the
mixing apparatus at an optimal temperature for the
components to be emulsified.
An emulsifying device according to the invention
comprises
- at least one mixing apparatus according to the
invention
- at least one motor for the stirrer units of the
mixing apparatus,
- at least two storage vessels for the phases to be
emulsified, which are connected to the mixing
apparatus by means of the inlet lines, and from

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which the components are fed air-free into the
mixing apparatus by means of conveying devices,
- at least one conveying device per component or per
component mixture,
- optionally input stream monitoring sensors and/or
output flow monitoring sensors, with which an
automatic quality control can optionally be
carried out simultaneously,
- optionally at least one device for temperature
control for the emulsifying device and the line
system for supply and removal of the components
and component mixtures,
- a control device for the monitoring and control of
the mixing apparatuses, the supply and removal of
the components and component mixtures,
- optionally a display device having an operating
panel for visualization and for the input of data.
Customarily, the emulsifying device, however,
comprises at least two mixing apparatuses, which are
connected one after the other and in which various
components are mixed with one another successively.
Here, the viscosity of the mixture produced in the
first mixing apparatus is always greater than or equal
to the viscosity in the following mixing apparatus(es).
At least the first mixing apparatus must correspond
here in construction and function to the at least one
mixing apparatus, i.e. in the first mixing apparatus
the particular flow management must be guaranteed, in
which the components are firstly mixed turbulently and
then achieve a lyotropic liquid-crystalline state by
means of passage through a percolating area.
In the production of conventional two-phase systems
such as WO emulsions, but also OW emulsions without a
gel network phase, in the emulsifying device according
to the invention the ratio of internal (disperse) phase
and external (continuous) phase in the first mixing

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apparatus is always greater than in the subsequent
mixing apparatus(es).
The entire system according to the invention is
controlled by means of a memory-programmable control.
This monitors, for example, the numbers of revolutions
of the mixing apparatuses, the inflow of the individual
components, the numbers of revolutions of the pumps,
the temperatures and pressures of the individual phases
added and all other parameters necessary for the
operation. It can in connection with mass or volume
flow meters monitor and control the inflow of the
individual components into the respective mixing
apparatuses. It can transmit previously defined
warnings and disorders by means of an optical or
acoustic output apparatus. Optical and visual output
can be located separately here from the apparatus
according to the invention such as, for example, in a
control center.
Alternative control possibilities, such as, for
example, SPS software or PC control, are likewise
possible as a combination of several control
possibilities.
By means of a remote maintenance module for the
connection of an analog telephone line or an ISDN line,
integrated with the control device or attached to this,
the access to a mobile radio network or a LAN or WLAN
network, it is possible to perform a remote maintenance
of the apparatus according to the invention or
alternatively to send warning and error messages or to
control the entire system according to invention.
Furthermore, the control can have a recipe module, in
which one or more recipes for various products are
deposited. Each recipe can in this connection consist
of a number of datasets. In the datasets, the

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parameters necessary for operation such as, for
example, the number of rotations, the ratio of the
volume flows etc., are held. After calling up of the
recipe, the datasets are executed either time-
controlled, or after triggering of a certain event,
e.g. the reaching of a certain temperature. This makes
possible the guarantee that products can be produced
with always the same quality.
The invention is illustrated more closely with the aid
of the following figures and working examples, without
restricting it. These show
Fig. 1 Emulsifying device containing a mixing
apparatus
Fig. 2 Various mixing apparatus geometries
Fig. 3 Various stirrer units
Fig. 4 Emulsifying device containing a mixing
apparatus with a further supply line in the
percolating area
Fig. 5 Emulsifying device containing two mixing
apparatuses
Fig. 6 Emulsifying device containing two mixing
apparatuses and a heat exchanger
Fig. 7 System scheme
Fig. 8 Energy diagram
Fig. 1 shows in sectional representation an
emulsifying device containing a mixing apparatus 1
having a rotationally symmetric chamber 2 sealed on all
sides in the form of a hollow cylinder. Into the

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chamber projects a stirrer shaft 10, on which are
arranged the stirrer wires 11, as shown in Fig. 3D. The
stirrer shaft 10 is driven by the motor 12 and guided
by the bearings and seals 8. Furthermore, the stirrer
shaft 10 is additionally guided in the bearing 9 in the
bottom part of the chamber 2. The chamber 2 has inlet
lines 5 or 6 in the lower part for the air-free supply
of the components A and B to be emulsified. In the
upper part of the chamber 2 is arranged the outlet line
7. Inlet and outlet lines are likewise temperature
controlled and have corresponding supply pumps (not
shown in Fig. 1).
The ratio between the distance between inlet lines 5
and 6 and outlet line 7 and the diameter of the chamber
2 is approximately 3.5.
The ratio between the distance between inlet lines 5
and 6 and outlet line 7 and the length of the stirrer
arms of the wire stirrers is approximately 15:1.
The chamber 2 is surrounded by a thermostat jacket 3,
which in combination with the thermostat 4 allows
temperature control of the mix. On account of the
greater distance between inlet and outlet compared to
the chamber diameter, the mix can be heated in a
controlled manner such that the energy input caused by
the stirrer does not destabilize the mix.
The emulsifying device according to Fig. 1 can be
utilized as follows, for example, for the dilution of
10C kg per hour of sodium lauryl ether sulfate (SLES):
By means of the pump of phase A, 41.4 kg per hour of
70% SLES is led continuously via the inlet line 5 and
by means of the pump of phase B 58.6 kg per hour of
water is led continuously via the inlet line 6 into the

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mixing apparatus 1 and mixed at 3000 revolutions per
min.
The mixing apparatus 1 is sealed on all sides and is
operated with exclusion of air. The components A and B
to be mixed are introduced into the chamber 2 of the
mixing apparatus 1 as flowable streams, mixed by means
of the stirrer unit 10 containing the stirrer wires 11
until the mixed components reach the outlet line 7 and
are led off such that no air penetrates into the
chamber 2 of the mixing apparatus 1.
On putting the mixing apparatus into operation, the air
contained therein is completely displaced within a
short time by the entering components A and B, whereby
the application of a vacuum is advantageously
unnecessary.
The mixed components A and B pass through the chamber 2
of the mixing apparatus 1 gradually beginning from the
inlet 5, 6 to the outlet 7. The components A and B
introduced into the chamber 2 via the inlet lines 5, 6
firstly migrate through an inlet-side turbulent mixing
area, in which they are turbulently mixed by the shear
forces exerted by the stirrer wires 11. In a
percolating mixing area connected above it, the
components are mixed further, the turbulent flow
decreasing and the viscosity increasing until a
lyotropic, lamellar liquid-crystalline phase
establishes in an outlet-side laminar mixing area. The
temperature of the mixture is kept constant by means of
the thermostat jacket 3.
28% strength SLES is obtained at the exit of the
stirring stage.
Fig. 4 shows in sectional representation a single-stage
emulsifying device, which is constructed and

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dimensioned analogously to Fig. 1, but has a further
inlet line 13 for a component C. Inlet and outlet lines
are temperature-controlled and are operatively
connected to pumps (not shown in Fig. 4).
The emulsifying device according to Fig. 4 can be
utilized as follows for the production of a simple O/W
spray.
Component A: aqueous emulsifier phase
Component B: oil phase
Component C: water phase
Component A is continuously introduced air-free at 8.1
kg per hour via the inlet line 5 and component B at
22.5 kg per hour via the inlet line 6 into chamber 2 of
the mixing apparatus 1 and mixed at approximately 3000
revolutions per min. The components A and B are mixed
by means of the stirrer unit 10 with the stirrer wires
11. After the mixture has passed through approximately
60% of the chamber length, the component C is metered
into the mixing chamber at 69.4 kg per hour via the
inlet line 13 and mixed until the mixed components
reach the outlet line 7. On putting into operation the
mixing apparatus 1, the air contained therein is
completely displaced by the entering components within
a short time, whereby the application of a vacuum is
advantageously unnecessary.
The mixed components A and B pass through the mixing
apparatus 1 gradually beginning from the inlet 5, 6 to
the outlet 7. The components A and B introduced via the
inlet lines 5, 6 into the chamber 2 firstly pass
through an inlet-side turbulent mixing area, in which
they are mixed turbulently by the shear forces exerted
by the stirrer wires 11. In a percolating mixing area
connected above it, the components A and B are further
mixed, the turbulent flow decreasing and the viscosity

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increasing until a lyotropic, liquid-crystalline phase
establishes in an outlet-side laminar mixing area and
in which the component C is supplied via the inlet line
13. The temperature of the mixture is kept constant by
means of the thermostat jacket 3.
Fig. 5 shows in sectional representation an
emulsifying device containing two mixing apparatuses 1
and 1'.
The emulsifying device according to Fig. 5 is
distinguished in that it consists of two mixing
apparatuses 1 and 1' connected in series, the outlet
line 7 of the first mixing apparatus 1 being connected
with the inlet line of the following mixing apparatus
1'. Each mixing apparatus 1 and 1' has a thermostat
jacket 3 or 3' and can be individually temperature
controlled, if desired, by means of the thermostat 4 or
4'. Stirrer elements are wire stirrers fixed to the
stirrer shaft according to the representation of Fig. 3
D.
The ratio between the distance between inlet lines 5
and 6 and outlet line 7 and the diameter of the chamber
2 of the mixing apparatus 1 is approximately 2Ø
The ratio between the distance between inlet lines 5
and 6 and outlet line 7 and the length of the stirrer
arms of the wire stirrers is 8:1.
Chamber 2' of the mixing apparatus 1' corresponds in
construction and dimensioning to the chamber 2 of the
mixing apparatus 1.
The mixing apparatuses 1 and 1' are equipped with
sensors for viscosity, pressure and temperature (not
shown here). The mixing apparatuses 1 and 1' are sealed
on all sides.

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The emulsifying device according to Fig. 5 can be
utilized as follows for the production of a simple OW
emulsion (120 kg per hour).
Component A: emulsifier with additional base for
neutralization of the thickener
Component B: oil phase
Component C: water phase with thickener
Component A is continuously introduced at 5.65 kg per
hour via the inlet line 5 and component B at 21.93 kg
per hour via the inlet line 6 into chamber 2 of the
mixing apparatus 1 and mixed at approximately 3000
revolutions per min. The components A and B are mixed
by means of the stirrer unit 10 with the stirrer wires
11 until the mixed components reach the outlet line 7
and are led off into the chamber 2' of the mixing
apparatus 1' such that no air penetrates into the
chamber 2 of the mixing apparatus 1. On putting into
operation the mixing apparatus 1 and 1', the air
contained therein is completely displaced by the
entering components within a short time, whereby the
application of a vacuum is advantageously unnecessary.
The mixed components A and B pass through the mixing
apparatus 1 gradually beginning from the inlet 5, 6 to
the outlet 7. The components A and B introduced via the
inlet lines 5, 6 into the chamber 2 firstly pass
through an inlet-side turbulent mixing area, in which
they are mixed turbulently by the shear forces exerted
by the stirrer wires 11. In a percolating mixing area
connected above it, the components A and B are further
mixed, the turbulent flow decreasing and the viscosity
increasing until a lyotropic, lamellar liquid-
crystalline phase establishes in an outlet-side laminar
mixing area. The temperature of the mixture is kept
constant by means of the thermostat jacket 3.

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Phase C is introduced into the chamber 2' at 72.42 kg
per hour together with the highly viscous mixture of
the components A and B via the inlet line 13. By means
of stirrer unit 10 and stirrer wires 11, the components
are mixed until they reach the outlet line 7' and are
led off such that no air penetrates into the chamber
21.
In the chamber 2', the highly viscous mixture of the
components A and B is diluted with the water phase of
the component C to give a flowable emulsion having a
particle size of 400 nm and a viscosity of 15 000 m
Pas. The thickener there serves for emulsion
stabilization and influences the skin sensation
positively.
Fig. 6 shows in sectional representation an
emulsifying device containing two mixing apparatuses 1
and 1' and an intermediately connected plate heat
exchanger 15. The emulsifying device according to Fig.
6 is constructed and dimensioned analogously to the
emulsifying device according to Fig. 5. The additional
inlet line 13 for the component C and the plate heat
exchanger 15 in the outlet line 7 to the inlet into
chamber 2 is different.
The emulsifying device according to Fig. 6 can be used
as follows for the production of a pearlescent agent
(100 kg per hour)
Component Component Vessel Throughput
temperature
A SLES room 22 kg per
temperature hour
(RT)
B glycol 70 C 24 kg per

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distearate hour
C water, betaine RT 21 kg per
(co-surfactant) hour
D water and RT 33 kg per
preservative hour
Temperature strand phase A: RT
Temperature strand phase B: 80 C
Temperature strand phase C: RT
Temperature strand phase D: RT
Temperature stirring stage 1 65 C
Temperature stirring stage 2: 5 C
Temperature heat exchanger: 40 C
Stirring stage 1: 3000 rpm
(Stirring stage 2: 3000 rpm
Component A is introduced at 22 kg per hour and at room
temperature continuously via the inlet line 5 and
component B is introduced at 24 kg per hour at a
temperature of 80 C via the inlet line 6 into the
chamber 2 of the mixing apparatus 1 and mixed at
approximately 3000 revolutions per min. The inlet line
6 is temperature controlled such that component B is
heated and is led into the chamber 2 at a temperature
of 80 C.

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When the components A and B mixed by means of the
stirrer unit 10 with the stirrer wires 11 reach the
area of the inlet line 13, the component C is fed into
the mixture at 21 kg per hour and a temperature of 65 C
via the inlet line 13. The thermostat jacket 3 of the
chamber 2' is temperature controlled at 65 C by means
of the thermostat 4 such that the components A, B and C
are mixed at 65 C.
After feeding in component C, the mixture passes over
to a percolating area until it reaches a lyotropic,
liquid-crystalline state in the area of the outlet line
7.
Before the lyotropic, liquid-crystalline mixture
removed via outlet line 7 is supplied to the chamber
2', this mixture is cooled to 40 C by means of the
plate heat exchanger 15 connected in the line 7'. This
is necessary, since the liquid-crystalline precursor,
which is prepared in the mixing apparatus 1, is
temperature-sensitive. The liquid-crystalline precursor
is then diluted with the phase D in the second mixing
apparatus it with counter cooling by the
heating/cooling jacket at a temperature of 5 C. The
product quality can only be achieved by maintaining
this temperature profile. If dilution with the cold
phase D was carried out above 40 C, the quality
requirements on the product could not be fulfilled. If
the product is cooled too deeply before diluting, a
product is likewise obtained that does not meet the
quality demands. This is owed to the fact that the
liquid-crystalline precursor assumes different liquid-
crystalline structures depending on the temperature,
from which different end states are achieved on
dilution.
In Fig. 7, a scheme of a complete emulsifying system
for the production of a shampoo is shown. The

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emulsifying system comprises 3 mixing apparatuses 1, 1'
and 111, storage containers A to D for the components A
to D to be mixed, connecting lines for the supply of
the components A to D to the appropriate mixing
apparatuses with associated pumps E, E', Ell, E''' and
valves, connecting lines for the removal of components,
thermostats 4, 4' and 4'' for the temperature control
of the mixing apparatuses 1, 1' and 111, a control
device (not shown in Fig. 7), which monitors and
regulates all process stages, a display device (not
shown in Fig. 7) with an operating part for the
visualization and input of process variables.
The connecting lines between the mixing apparatuses 1
and 1' and also 1' and 1'' are equipped with
temperature sensors T for the temperature control of
the mixing chambers.
The mixing apparatuses and connecting lines have
sensors for product and process control (not shown in
Fig. 7).
Furthermore, the outlet lines of the individual mixing
apparatuses can have further sensors, which, for
example, make possible continuous particle size
measurement, directly or in a bypass, a temperature
measurement, a pressure measurement or the like.
The system according to Fig. 7 is explained with the
aid of an emulsifying example for the production of a
shampoo.
The following components are stored in the storage
tanks:
component A: sodium laureth sulfate (SLES) 700
component B: water, preservative, co-surfactant
component C: pearlescent agent
component D: water, salt, colorants

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The three mixing apparatuses 1, 1', 1'' which are in
each case equipped with a thermostat jacket and have
their own heating/cooling circuit form the core
constituents. In the mixing apparatus 1, a highly
viscous gel phase is produced from the individual
components (component A, component B, component C). The
mixing apparatus 1' serves for the subsequent stirring
of the gel phase which then led to the mixing apparatus
111, to be diluted there with component D.
Component A, component B and component C are aspirated
using eccentric spiral pumps E, E' and E'' and supplied
to the first mixing apparatus 1' in the ratio 1:
3.71:0.36. The component D is supplied to the mixing
apparatus 1'' using the pump E''' in the ratio 2.21
based on component A. The pumps were selected such that
they supply a uniform, non-pulsing component flow. Each
pump must supply a minimal stable supply stream that is
sufficient for a total production amount of 100 kg to
300 kg per hour. Eccentric spiral pumps are very highly
suitable in the scheme shown, since they are uncritical
with regard to changing viscosities.
On account of the fact that in the system shown
schematically in Fig. 7, no flow meters for the
individual product streams are present, advantageously
a pump is to be chosen which has a linear transport
characteristic line. Thus changing transport rates can
be calculated simply. In systems with flow meters
(volume or mass), nonlinear pumps such as, for example,
gear wheel pumps can also be employed without problem.
The pumps E are designed for a counter pressure of up
to 5 bar. By means of the exits component A to
component D, the transport amount of the respective
pump can be determined simply at a set speed of
rotation. The determination of the transport amount at

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100 rpm offers itself here. The corresponding transport
stream is captured and weighed in a previously tared
vessel for the period of 1 min. This process is
repeated three times and the mean value is formed from
all three transport streams. The transport stream of
the pump thus averaged can then be converted by means
of the three set to the desired transport stream needed
for the recipe.
Using the speeds thus determined, the pumps and the
motors of the stirrer units are now started. The pumps
transport only the required amounts of the individual
components to the mixing apparatuses in order to obtain
the final product. By means of the built-in pressure
sensors P, the resulting pressure can be controlled,
and in the case of overpressure in the pipeline or the
mixing apparatuses the control can react accordingly
and emit a warning, stop the system, or take similar
countermeasures. By means of the temperature sensors
integrated into the outlet lines of the individual
mixing apparatuses, the product temperature can be
determined and utilized for controlling the temperature
control equipment of the double jacket or otherwise
processed in the control or a peripheral apparatus.
In the production of the shampoo, the total efficiency
of the complete system was measured as a function of
total flow.
The total power consumption was measured at a
throughput of 100 kg/hour, 150 kg/hour, 200 kg/hour,
250 kg/hour, 300 kg/hour and 400 kg/hour. The
measurements determined were plotted in an XY graph
(Fig. 8).
Conditions:
Emulsifying system having 3 mixing chambers

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Chamber diameter: 50 mm
Stirring tool: part-wire stirrer

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Measured values:
Throughput [kg/h] Energy consumption [kW]
100 1.08
150 1.13
200 1.17
250 1.26
300 1.25
400 1.28
If the values are extrapolated with the aid of a
statistics program, even with a throughput of 10 000
kg/h a total energy requirement of 2 kW is not
exceeded.

Dessin représentatif
Une figure unique qui représente un dessin illustrant l'invention.
États administratifs

2024-08-01 : Dans le cadre de la transition vers les Brevets de nouvelle génération (BNG), la base de données sur les brevets canadiens (BDBC) contient désormais un Historique d'événement plus détaillé, qui reproduit le Journal des événements de notre nouvelle solution interne.

Veuillez noter que les événements débutant par « Inactive : » se réfèrent à des événements qui ne sont plus utilisés dans notre nouvelle solution interne.

Pour une meilleure compréhension de l'état de la demande ou brevet qui figure sur cette page, la rubrique Mise en garde , et les descriptions de Brevet , Historique d'événement , Taxes périodiques et Historique des paiements devraient être consultées.

Historique d'événement

Description Date
Le délai pour l'annulation est expiré 2022-11-08
Lettre envoyée 2022-05-06
Inactive : CIB expirée 2022-01-01
Inactive : CIB expirée 2022-01-01
Inactive : CIB expirée 2022-01-01
Inactive : CIB expirée 2022-01-01
Inactive : CIB expirée 2022-01-01
Lettre envoyée 2021-11-08
Inactive : Certificat d'inscription (Transfert) 2021-09-03
Inactive : Transfert individuel 2021-08-18
Requête pour le changement d'adresse ou de mode de correspondance reçue 2021-08-18
Lettre envoyée 2021-05-06
Représentant commun nommé 2019-10-30
Représentant commun nommé 2019-10-30
Accordé par délivrance 2017-03-14
Inactive : Page couverture publiée 2017-03-13
Préoctroi 2017-01-31
Inactive : Taxe finale reçue 2017-01-31
Un avis d'acceptation est envoyé 2017-01-03
Lettre envoyée 2017-01-03
Un avis d'acceptation est envoyé 2017-01-03
Inactive : Approuvée aux fins d'acceptation (AFA) 2016-12-21
Inactive : Q2 réussi 2016-12-21
Modification reçue - modification volontaire 2016-09-07
Inactive : Dem. de l'examinateur par.30(2) Règles 2016-04-18
Inactive : Rapport - Aucun CQ 2016-04-14
Modification reçue - modification volontaire 2016-01-07
Inactive : Dem. de l'examinateur par.30(2) Règles 2015-07-07
Inactive : Rapport - Aucun CQ 2015-06-23
Lettre envoyée 2014-05-29
Toutes les exigences pour l'examen - jugée conforme 2014-05-23
Exigences pour une requête d'examen - jugée conforme 2014-05-23
Requête d'examen reçue 2014-05-23
Inactive : Lettre officielle 2013-11-26
Demande de correction du demandeur reçue 2013-06-07
Modification reçue - modification volontaire 2013-01-14
Inactive : Page couverture publiée 2013-01-09
Inactive : CIB en 1re position 2012-12-28
Inactive : Notice - Entrée phase nat. - Pas de RE 2012-12-28
Inactive : CIB attribuée 2012-12-28
Inactive : CIB attribuée 2012-12-28
Inactive : CIB attribuée 2012-12-28
Inactive : CIB attribuée 2012-12-28
Inactive : CIB attribuée 2012-12-28
Demande reçue - PCT 2012-12-28
Exigences pour l'entrée dans la phase nationale - jugée conforme 2012-11-06
Demande publiée (accessible au public) 2011-11-10

Historique d'abandonnement

Il n'y a pas d'historique d'abandonnement

Taxes périodiques

Le dernier paiement a été reçu le 2016-03-17

Avis : Si le paiement en totalité n'a pas été reçu au plus tard à la date indiquée, une taxe supplémentaire peut être imposée, soit une des taxes suivantes :

  • taxe de rétablissement ;
  • taxe pour paiement en souffrance ; ou
  • taxe additionnelle pour le renversement d'une péremption réputée.

Veuillez vous référer à la page web des taxes sur les brevets de l'OPIC pour voir tous les montants actuels des taxes.

Historique des taxes

Type de taxes Anniversaire Échéance Date payée
Taxe nationale de base - générale 2012-11-06
TM (demande, 2e anniv.) - générale 02 2013-05-06 2012-11-06
TM (demande, 3e anniv.) - générale 03 2014-05-06 2014-04-21
Requête d'examen - générale 2014-05-23
TM (demande, 4e anniv.) - générale 04 2015-05-06 2015-04-20
TM (demande, 5e anniv.) - générale 05 2016-05-06 2016-03-17
Taxe finale - générale 2017-01-31
TM (brevet, 6e anniv.) - générale 2017-05-08 2017-05-01
TM (brevet, 7e anniv.) - générale 2018-05-07 2018-04-27
TM (brevet, 8e anniv.) - générale 2019-05-06 2019-04-29
TM (brevet, 9e anniv.) - générale 2020-05-06 2020-04-27
Enregistrement d'un document 2021-08-18 2021-08-18
Titulaires au dossier

Les titulaires actuels et antérieures au dossier sont affichés en ordre alphabétique.

Titulaires actuels au dossier
CLARIANT PRODUKTE (DEUTSCHLAND) GMBH
Titulaires antérieures au dossier
ANDREAS JUNG
GERD DAHMS
HENDRIK DOERR
Les propriétaires antérieurs qui ne figurent pas dans la liste des « Propriétaires au dossier » apparaîtront dans d'autres documents au dossier.
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Description du
Document 
Date
(aaaa-mm-jj) 
Nombre de pages   Taille de l'image (Ko) 
Revendications 2016-09-07 3 92
Description 2012-11-06 39 1 448
Revendications 2012-11-06 4 120
Abrégé 2012-11-06 1 10
Dessins 2012-11-06 8 170
Dessin représentatif 2013-01-09 1 11
Page couverture 2013-01-09 1 41
Revendications 2016-01-07 3 93
Page couverture 2017-02-13 1 37
Dessin représentatif 2017-02-13 1 7
Avis d'entree dans la phase nationale 2012-12-28 1 206
Accusé de réception de la requête d'examen 2014-05-29 1 175
Avis du commissaire - Demande jugée acceptable 2017-01-03 1 164
Avis du commissaire - Non-paiement de la taxe pour le maintien en état des droits conférés par un brevet 2021-06-17 1 558
Courtoisie - Certificat d'inscription (transfert) 2021-09-03 1 411
Courtoisie - Brevet réputé périmé 2021-11-29 1 549
Avis du commissaire - Non-paiement de la taxe pour le maintien en état des droits conférés par un brevet 2022-06-17 1 543
PCT 2012-11-06 16 515
PCT 2013-01-14 8 233
Correspondance 2013-06-07 2 86
Correspondance 2013-11-26 1 14
Demande de l'examinateur 2015-07-07 4 274
Modification / réponse à un rapport 2016-01-07 10 331
Taxes 2016-03-17 1 26
Demande de l'examinateur 2016-04-18 4 260
Modification / réponse à un rapport 2016-09-07 10 375
Taxe finale 2017-01-31 1 43
Paiement de taxe périodique 2017-05-01 1 26
Changement à la méthode de correspondance 2021-08-18 3 73